ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Dimethylformamide → 2-Difluoromethoxy-6-propylsulfanylbenzonitrile

HRID 229935
ノート
印刷プレビュー

反応式

HRID 229935 の反応式
[F:1][CH:2]([F:13])[O:3][C:4]1[CH:11]=[CH:10][CH:9]=[C:8](F)[C:5]=1[C:6]#[N:7].CN(C)C=O.[CH2:19]([SH:22])[CH2:20][CH3:21].[OH-].[K+]>O>[F:1][CH:2]([F:13])[O:3][C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([S:22][CH2:19][CH2:20][CH3:21])[C:5]=1[C:6]#[N:7]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 7848Propyl mercaptanHCID 14797Potassium HydroxideHCID 234483612-(Difluoromethoxy)-6-fluorobenzonitrile

生成物 1

HCID 685651162-Difluoromethoxy-6-propylsulfanylbenzonitrile収率 76%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

180 g (0.96 mol) 2-difluoromethoxy-6-fluorobenzonitrile were introduced into 1.5 l of dimethylformamide at room temperature. 73.2 g (0.96 mol) of propanethiol were added dropwise and, after cooling to 0° C., 70 g (1.25 mol) of potassium hydroxide pellets, dissolved in 600 ml of water, were added dropwise at 0° C. The mixture was stirred for one hour and then warmed to room temperature. The reaction mixture was stirred into 3.5 l of ice-water and extracted three times with 500 ml of methyl tert.-butyl ether. The combined organic phases were washed twice with 500 ml of 1N hydrochloric acid and dried over sodium sulfate. Then, the solvent was distilled off in vacuo. The oil obtained was distilled in vacuo (b.p.: 180-185° C./0.5 mbar). Yield: 76% of theory.

後処理

  1. additionwere added dropwise at 0° C
  2. temperaturewarmed to room temperature
  3. extractionextracted three times with 500 ml of methyl tert.-butyl ether
  4. washThe combined organic phases were washed twice with 500 ml of 1N hydrochloric acid
  5. dry with materialdried over sodium sulfate
  6. distillationThen, the solvent was distilled off in vacuo
  7. customThe oil obtained
  8. distillationwas distilled in vacuo (b.p.: 180-185° C./0.5 mbar)

出典と根拠

ORDレコード
ord-9eef223353e64379bcb80fd4f526eb3d
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07563921B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート